CN112853120B - LiHCO is leached in old and useless lithium cell recovery 3 Solution deep defluorination method - Google Patents
LiHCO is leached in old and useless lithium cell recovery 3 Solution deep defluorination method Download PDFInfo
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- CN112853120B CN112853120B CN202011636165.XA CN202011636165A CN112853120B CN 112853120 B CN112853120 B CN 112853120B CN 202011636165 A CN202011636165 A CN 202011636165A CN 112853120 B CN112853120 B CN 112853120B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
- C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
Abstract
The invention belongs to the technical field of lithium ion battery recovery, and provides a method for recovering LiHCO from waste lithium ion batteries 3 Solution deep defluorination method using LiHCO 3 And preparing the battery grade lithium carbonate by taking the solution as the stock solution. The method comprises the following steps: A. preparing raw materials; B. alkali washing of the fluorine removing agent; B. CO ventilation 2 Regulating and controlling the pH of the system; liHCO 3 Removing fluorine from the solution; E. regenerating the defluorinating agent. The invention is realized by the method of preparing LiHCO 3 Adding fluorine removing agent containing aluminum, titanium, zirconium, nitrogen and other elements into the solution, and bubbling CO 2 The reaction pH is regulated and controlled by gas, so that the deep defluorination effect can be achieved, and LiHCO can be ensured 3 The solution system is unchanged, and meanwhile, new impurities are not introduced, so that the preparation requirement of the subsequent battery-grade lithium carbonate is met, and the product quality is improved.
Description
Technical Field
The invention relates to the technical field of battery recovery, in particular to a defluorination method for recovering leaching liquid from waste lithium batteries.
Background
In recent years, the number of lithium ion batteries used has increased exponentially, accompanied by a synchronous increase in the number of obsolete batteries. The lithium ion battery contains high added value metals such as cobalt, nickel, manganese, lithium and the like. If not recovered, not only resources are wasted, but also substances such as electrolyte contained in the battery are extremely liable to cause environmental pollution. Therefore, the battery needs to be effectively recycled, and the recycling of resources is realized. In the process of purifying and separating each valuable element in the lithium ion battery, aluminum foil, copper foil and battery electrode powder often exist, the aluminum foil, the copper foil and the battery electrode powder cannot be completely separated, fluorine in electrolyte enters into leaching liquid along with leaching, and the fluorine content in subsequent products is high. In the current recovery process of waste batteries, after the lithium ion batteries are crushed and sieved, the obtained battery powder is subjected to leaching, impurity removal and extraction to recover valuable metals, and the defluorination is mainly carried out in the later stage of the recovery process. Disadvantages of the latter stage defluorination include: (1) In the recovery process of valuable metals, the concentration of various ions in the wastewater can be gradually increased, so that the effect of the later-stage defluorination is poor, the consumption of auxiliary materials is increased, a large amount of salt is entrained in defluorination residues, and the residue amount is increased; (2) Fluorine in the lithium ion battery enters a solution along with various metals in a leaching process, so that equipment corrosion can be accelerated; (3) The fluoride ions and other ions in the solution can form stable compounds, which easily cause pipeline blockage; (4) Fluorine enters the strip liquor of P-204 in the extraction section, and is continuously enriched and circulated, so that the fluorine is entrained into the product in the extraction process, and the product quality is affected. Therefore, the above-mentioned problems can be avoided by subjecting the battery powder leaching solution to a defluorination treatment.
The current mature defluorination methods include chemical precipitation, activated alumina adsorption, ion exchange resin, etc. In the precipitation method, calcium salt is a relatively wide-range defluorination reagent and is utilized to generate insoluble CaF 2 The defluorination effect is achieved. The battery powder is subjected to roasting reduction and carbonization leaching to obtain LiHCO 3 Solution for ensuring LiHCO 3 The solution system is unchanged, the introduction of calcium salt impurities is avoided, the preparation of battery-grade lithium carbonate is influenced, a small amount of calcium salt is added according to calculation of the Ksp constant of calcium fluoride, and the defluorination effect is not ideal. Thus, in LiHCO 3 The calcium salt is added into the solution to only achieve the purposes of coarse defluorination and deep defluorination, and the quality of the battery-grade lithium carbonate is affected. The existing adsorptive defluorinating agent has better defluorinating effect basically under the acidic condition and has poor defluorinating effect under the alkaline condition. Thus, the existing defluorinating agent is adopted to carry out the process of slightly alkaline LiHCO 3 The solution has poor defluorination effect.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for deeply removing fluorine from a waste lithium battery recovery leaching solution, which can achieve the purpose of deeply removing fluorine and can not introduce new pollution factors.
For the purpose ofThe method achieves the aim, and the method for recycling and leaching the LiHCO from the waste lithium battery 3 The method for deeply removing fluorine in the solution specifically comprises the following steps:
A. raw material preparation: taking a certain amount of waste battery material to carbonize and presoak to prepare LiHCO 3 Solution according to LiHCO 3 Adding 5% -20% fluorine removing agent, namely 1000mLLiHCO 3 Adding 50 g-200 g of defluorinating agent into the solution; the defluorinating agent is an acid activated composite material prepared from aluminum oxide, butyl titanate, zirconium sulfate and a nitrogen-containing compound;
B. alkali washing defluorinating agent: mixing and stirring the defluorinating agent and inorganic base according to a certain solid-to-liquid ratio, and filtering to obtain the defluorinating agent for eluting chlorine radicals or sulfate radicals;
C. adjusting the pH value of a system: adding the defluorinating agent obtained in the step B into LiHCO 3 In the solution, then CO is introduced 2 Regulating the pH value of the reaction system to 7-8;
D.LiHCO 3 solution defluorination: stirring and reacting while blowing air at room temperature, and then press-filtering to obtain LiHCO 3 Fluorine-removing liquid and fluorine-containing slag;
E. regenerating the defluorinating agent: and D, adding sodium hydroxide solution into the fluorine-containing slag obtained in the step D according to a certain solid-to-liquid ratio, reacting at a certain temperature, and performing filter pressing, washing and re-filter pressing after the reaction is completed to obtain the regenerated fluorine removing agent.
Further, the fluorine removing agent in the step A is CF-2000 fluorine removing agent produced by Changsha Huasheng new material science and technology Co., ltd.
Further, the inorganic alkali in the step B is sodium hydroxide, and the solid-liquid ratio is 1:2-5.
Further, the stirring reaction time in the step D is 0.5-1.5 h.
Further, the mass fraction of the sodium hydroxide solution in the step E is 2% -5%, the solid-liquid ratio of the fluorine-containing slag and the sodium hydroxide solution is 1:3-6, the reaction temperature is 25-50 ℃, and the reaction time is 0.5h.
The acid activated defluorinating agent is subjected to alkali washing, so that a great amount of chloride and sulfate radical of a system cannot be introduced in the defluorination process to cause LiHCO 3 The solution system changes. Titanium in the defluorinating agent provides adsorption activity, aluminum oxide provides a matrix, and zirconium sulfate provides dispersibility.
The invention introduces CO in the defluorination stage 2 Gas, liHCO 3 CO is introduced into the solution 2 Can not only achieve the control of pH in the defluorination stage, but also avoid LiHCO 3 The low-fluorine (less than 0.02%) battery grade lithium carbonate can be prepared in one step. If the pH is controlled by directly adding acid, liHCO is prepared 3 Conversion of the System to Li 2 SO 4 LiCl system. And is introduced with CO 2 No new impurity is introduced, and the preparation requirement of the subsequent battery grade lithium carbonate is met.
Fluorine is absorbed under the acidic condition, the basic defluorination is carried out, and the lower the pH value is, the better the defluorination effect is; but can lead to LiHCO while regulating pH by adding acid 3 The solution system changes. The invention not only improves the defluorination efficiency, but also ensures LiHCO 3 The solution system is unchanged, fluorine removing agents containing elements such as aluminum, titanium, zirconium, nitrogen and the like are adopted, and CO is introduced in the fluorine removing stage 2 The pH value of the reaction system is regulated to 7-8, so that the purpose of high-efficiency fluorine removal in a weak alkaline environment is realized.
Detailed Description
Example 1:
A. raw material preparation: taking 1L of waste battery material to carbonize and presoak to prepare LiHCO 3 The solution, measured as LiHCO, had a fluoride ion content of 110ppm 3 Adding 15% fluorine removing agent, namely 1000mLLiHCO 3 150g of fluorine scavenger was added to the solution. The fluorine removing agent is CF-2000 fluorine removing agent produced by Changsha Huasheng new material science and technology Co-ordination.
B. Alkali washing of fluorine removing agent: adding 2% NaOH solution into the fluorine removing agent according to the solid-to-liquid ratio of 1:2, mixing, stirring, reacting for 0.5h, and filtering to obtain the eluted sulfate radical or chloride ion fluorine removing agent.
C. Adjusting the pH value of a system: adding the washed defluorinating agent into LiHCO 3 Introducing CO into the solution 2 The pH of the system was adjusted to 7.25.
D.LiHCO 3 Solution defluorination: stirring for 1h while blowing air, and vacuum filtering to obtain fluorine-containing slag and LiHCO after defluorination 3 The solution is prepared into a liquid preparation,measurement of LiHCO after defluorination 3 The fluoride ion content of the solution was 3.8ppm.
E. Regenerating the defluorinating agent: adding 2% sodium hydroxide solution into the fluorine-containing slag according to the solid-to-liquid ratio of 1:3, reacting for 0.5h at room temperature, and then carrying out suction filtration, washing with deionized water and suction filtration to obtain the fluorine-removing agent.
F. Regenerated defluorinating agent for defluorination: repeating the steps A-D of example 1 with the regenerated fluorine scavenger for LiHCO having a fluoride ion content of 110ppm 3 Solution defluorination, liHCO after defluorination is measured 3 The fluoride ion content of the solution was 4.1ppm.
Example 2:
A. raw material preparation: taking 1L of waste battery material to carbonize and presoak to prepare LiHCO 3 The solution, measured as LiHCO, had a fluoride ion content of 88.5ppm 3 Adding 10% fluorine removing agent, namely 1000 ml_ iHCO 3 100g of fluorine scavenger was added to the solution. The fluorine removing agent is CF-2000 fluorine removing agent produced by Changsha Huasheng new material science and technology Co-ordination.
B. Alkali washing of fluorine removing agent: adding 2% NaOH solution into the fluorine removing agent according to the solid-to-liquid ratio of 1:3, mixing, stirring, reacting for 0.5h, and filtering to obtain the eluted sulfate radical or chloride ion fluorine removing agent.
C. Adjusting the pH value of a system: adding the washed defluorinating agent into LiHCO 3 Introducing CO into the solution 2 The pH of the system was adjusted to 7.32.
D.LiHCO 3 Solution defluorination: stirring for 1h while blowing air, and vacuum filtering to obtain fluorine-containing slag and LiHCO after defluorination 3 Solution, liHCO after defluorination was measured 3 The fluoride ion content of the solution was 5.86ppm.
E. Regenerating the defluorinating agent: adding 2% sodium hydroxide solution into the fluorine-containing slag according to the solid-to-liquid ratio of 1:3, reacting for 0.5h at room temperature, and then carrying out suction filtration, washing with deionized water and suction filtration to obtain the fluorine-removing agent.
F. Regenerated defluorinating agent for defluorination: the procedure A-D of example 2 was repeated for LiHCO having a fluoride ion content of 88.5ppm with the regenerated fluorine scavenger 3 Solution defluorination, liHCO after defluorination is measured 3 The fluoride ion content of the solution was 5.75ppm.
Example 3:
A. raw material preparation: taking outLiHCO prepared by carbonizing and presoaking 1L waste battery material 3 The solution, measured as LiHCO, had a fluoride ion content of 88.5ppm 3 Adding 5% fluorine removing agent, namely 1000 ml_ iHCO 3 50g of fluorine scavenger was added to the solution. The fluorine removing agent is CF-2000 fluorine removing agent produced by Changsha Huasheng new material science and technology Co-ordination.
B. Alkali washing of fluorine removing agent: adding 2% NaOH solution into the fluorine removing agent according to the solid-to-liquid ratio of 1:4, mixing, stirring, reacting for 0.5h, and filtering to obtain the eluted sulfate radical or chloride ion fluorine removing agent.
C. Adjusting the pH value of a system: adding the washed defluorinating agent into LiHCO 3 Introducing CO into the solution 2 The pH of the system was adjusted to 7.62.
D.LiHCO 3 Solution defluorination: stirring for 1h while blowing air, and vacuum filtering to obtain fluorine-containing slag and LiHCO after defluorination 3 Solution, liHCO after defluorination was measured 3 The fluoride ion content of the solution was 3.23ppm.
E. Regenerating the defluorinating agent: adding 2% sodium hydroxide solution into the fluorine-containing slag according to the solid-to-liquid ratio of 1:3, reacting for 0.5h at room temperature, and then carrying out suction filtration, washing with deionized water and suction filtration to obtain the fluorine-removing agent.
F. Regenerated defluorinating agent for defluorination: repeating the steps A-D of example 3 with the regenerated fluorine scavenger for LiHCO having a fluoride ion content of 88.5ppm 3 Solution defluorination, liHCO after defluorination is measured 3 The fluoride ion content of the solution was 3.75ppm.
Claims (4)
1. A method for deeply removing fluorine from LiHCO3 solution by recycling and leaching waste lithium batteries is characterized by comprising the following steps of: the method comprises the following steps:
A. raw material preparation: taking a certain amount of LiHCO3 solution prepared by carbonizing and presoaking waste battery materials, and adding 5% -20% of fluorine removing agent according to the volume of the LiHCO3 solution, namely adding 50-200 g of fluorine removing agent into 1000mLLiHCO3 solution; the defluorinating agent is an acid activated composite material prepared from aluminum oxide, butyl titanate, zirconium sulfate and a nitrogen-containing compound;
B. alkali washing defluorinating agent: mixing and stirring the defluorinating agent and inorganic base according to a certain solid-to-liquid ratio, and filtering to obtain the defluorinating agent for eluting chlorine radicals or sulfate radicals;
C. adjusting the pH value of a system: adding the defluorinating agent obtained in the step B into LiHCO3 solution, then introducing CO2, and regulating the pH value of a reaction system to 7-8;
LiHCO3 solution defluorination: stirring and reacting while blowing air at room temperature, and then performing filter pressing to obtain LiHCO3 defluorination liquid and fluorine-containing slag;
E. regenerating the defluorinating agent: and D, adding sodium hydroxide solution into the fluorine-containing slag obtained in the step D according to a certain solid-to-liquid ratio, reacting at a certain temperature, and performing filter pressing, washing and re-filter pressing after the reaction is completed to obtain the regenerated fluorine removing agent.
2. The method for deeply removing fluorine from a solution of LiHCO3 leached from a waste lithium battery according to claim 1, which is characterized by comprising the following steps: the inorganic alkali in the step B is sodium hydroxide, and the solid-liquid ratio is 1:2-5.
3. The method for deeply removing fluorine from a solution of LiHCO3 leached from a waste lithium battery according to claim 1, which is characterized by comprising the following steps: and D, stirring and reacting for 0.5-1.5 h.
4. The method for deeply removing fluorine from a solution of LiHCO3 leached from a waste lithium battery according to claim 1, which is characterized by comprising the following steps: and E, the mass fraction of the sodium hydroxide solution in the step is 2-5%, the solid-liquid ratio of the fluorine-containing slag and the sodium hydroxide solution is 1:3-6, the reaction temperature is 25-50 ℃, and the reaction time is 0.5h.
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CN113802006A (en) * | 2021-08-30 | 2021-12-17 | 广东邦普循环科技有限公司 | Method for removing copper fluoride from battery powder leachate |
CN114214517B (en) * | 2021-10-26 | 2023-07-07 | 广东邦普循环科技有限公司 | Method for removing fluorine in lithium battery positive electrode leaching solution |
CN115849415B (en) * | 2023-03-02 | 2023-05-02 | 矿冶科技集团有限公司 | Method for preparing battery grade lithium carbonate |
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CN108311095A (en) * | 2018-03-16 | 2018-07-24 | 锡林郭勒职业学院 | A kind of preparation method and applications of flyash defluorinating agent |
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